BCRE Lab Manual

Biochemical Reaction Engineering Lab Manual
Department of Biotechnology
Vignan’s Foundation for Science, Technology and Research

(Deemed to be University)
Department of Biotechnology
Biochemical Reaction Engineering

III Year B.Tech Biotechnology
List of Experiments
Exp
Name of the experiment COs Mapped PSO
t No
1 Kinetic Studies in batch reactor with equimolar feed CO1, CO2,CO7, PSO1
2 Kinetic Studies in batch reactor with non-equimolar feed CO1, CO2, CO3 PSO1
3 Kinetic studies in Mixed flow reactor CO2,CO4,CO9 PSO1
4 Kinetic Studies in Plug flow reactor CO2,CO4,CO9 PSO1
5 Kinetic Studies in Isothermal Batch reactor CO2, CO4,CO7 PSO1
6 Kinetic Studies in Adiabatic reactor CO1, CO2,CO7 PSO1
7 RTD studies in Mixed flow reactor CO3, CO2,CO9 PSO1
8 RTD studies in Mixed flow reactors in series CO2,CO4,CO10 PSO1
9 RTD studies in Plug flow reactor CO1, CO2,CO7 PSO1
10 RTD studies in Combined reactor CO1, CO2,CO7 PSO1
Faculty Incharge
Vision of the Institution:
To evolve into a center of excellence in Science and Technology through creative and innovative
practices in teaching-learning, towards promoting academic achievement & research excellence
to produce internationally accepted, competitive and world class professionals who are
psychologically strong and emotionally balanced imbued with social consciousness and ethical
values.
Mission of the Institution:
To provide high quality academic programmes, training activities, research facilities and
opportunities supported by continuous industry –institute interaction aimed at promoting
employability, entrepreneurship, leadership and research aptitude among students and
contribute to the economic and technological development of the region, state and nation.
Vision and Mission of the Program

Vision
To be a Centre of Excellence in the field of Biotechnology with high quality academics and the
State-of-the art research to produce multifaceted, internationally accepted employable
professionals.
Mission
M1: Providing the State-of-the art curriculum with skill based practices in teaching and
learning to pursue career opportunities in biological and bioprocess related fields.
M2: Offering adequate laboratory facilities with conducive research vicinity to make students
ready for industry and update to pursue higher education, research and consultancy.
M3: Transforming into committed professionals with sense of belonging, leadership abilities,
managerial competencies, team participation, social awareness, human values and ethics.
Course Description and Objective:

This course offers the knowledge on various reaction types and its kinetics. The objective of this
course is to provide students adequate knowledge about understanding kinetics and predict
performance equation for various reactors and its design.
OBJECTIVES:
1. To understand various reaction types and its kinetics.
2. To predict performance equation for various reactors.
3. To develop growth kinetics.
4. To study multiple reactions.
5. To design various bioreactors.
Course Outcomes
The student will be able to:
CO1: Understand various reactions and its kinetics
CO2: Apply growth kinetics to reactor design.
CO3: Analyze product distribution in multiple reactions.
CO4: Develop performance equation for various reactors.
CO5: Diagnosis ills of bioreactor.
CO6: Design bioreactor.
Skills to be attained:
1. Searching reaction mechanism for non-elementary reactions.
2. Estimation of rate of reaction, rate constant and order for given reactions.
3. Prediction of ills of reactor.
4. Design of bioreactor.
5. Analysis of product distribution in multiple reactions.
EXPERIMENT – I
KINETIC STUDIES IN BATCH REACTOR EQUIMOLAR FEED
AIM:
To determine rate constant for the saponification by using Equimolar feed.
APPARATUS:
Reactor vessel with stirrer, Conical flasks, Burette, Pipette.
CHEMICALS REQUIRED:
NaOH solution, Ethyl Acetate, Hydrochloric acid, Phenolphthalein indicator
THEORY:
The experimental batch reactor is usually operated isothermally and at constant volume, because it is easy
to interpret the results of such runs. This reactor id relatively simple device adaptable to small - scale
laboratory set-ups, and it needs but little auxiliary equipment or instrumentation. Thus, it is used whenever
possible for obtaining homogeneous data. The starting point for all design is the material balance expressed for
any reactant or product over a small element of volume.
Element of reactor volume
Reactants enters Reactants leaves
Reactant accumulates Reactant disappears by
within the element reaction within the element

Rate of Rate of Rate of reactant Rate of
reactant flow reactant flow loss due to accumulation of
into element = +
out of element +
chemical reactant within
of volume of volume reaction within the element of
= + the element of +
volume
volume
If the composition within the reactor is uniform (independent of position), the accounting may be
made over the whole reactor. If the composition is not uniform (dependent on position), it must be
made over a differential element of volume and then integrated across the whole reactor for the
appropriate flow and concentration conditions.
INPUT = OUTPUT + DISAPPEARNCE BY REACTION + ACCUMULATION ----------(1)
In the batch reactor of figure 1.1 the reactants are initially charged into a container, are well mixed,
and are left to react for a certain period. The resultant mixture is then discharged. This is unsteady
state operation where the concentration changes with time. The concentration is independent of
position, so we can make material balance over the entire reactor.
Make a material balance for any component A. For such an accounting we usually select the
limiting reactant.
Input = 0
Output = 0
Disappearance by reaction ( moles / time ) = ( -A ) V

dN A d [ N AO (1− X A )] dX A
N AO
Accumulation of A ( moles / time ) = dt = dt = - dt
By replacing these terms in equation (1)
dX A
N AO
0 = 0 + ( -A ) V - dt
dX A
N AO
( -A ) V = dt ----------------------------------------(2)
Rearranging and integrating equation (2) gives
XA
dX A
N AO ∫
t= 0 (−γ A )V ----------------------------(3)
for constant volume reactions
XA
dX A
t=C AO ∫
0 (−γ A ) -----------------------------------------(4)
The performance equation for Constant volume batch reactor is
XA
dX A
t=C AO ∫
0 (−γ A )
Consider a second order irreversible bi-molecular elementary reaction given below
A + B Products
The rate equation for above reaction is -A = K CA CB (5)

-----------------------
Let XA and XB are conversions of A and B at any time, the concentrations of A and B at any time in
the reactor are
CA = CAO ( 1 - XA ) CB = CBO ( 1 – XB )
Substitute above expressions in equation (5)
-A = K CAO ( 1 - XA ) CBO ( 1 – XB )
Rearrange above equation
-A = K CAO ( 1 - XA ) (CBO – CBO XB ) --------------------------------------------(6)
at any time moles of B reacted is equal to moles of B reacted
moles of B reacted = CBO XB
moles of A reacted = CAO XA
CBO XB = CAO XA ----------------------------------------------------(7)
Substitute (7) in (6)
-A = K CAO ( 1 - XA ) (CBO – CAO XA )
For equimolar feed CAO = CBO M = 1
-A = K CAO2 ( 1 - XA )2 ---------------------------------------(8)
Substitute equation (8) in equation (4)
XA
dX A
t =C AO ∫
0 KC ( 1 - XA )2
AO2
Integration of above equation leads to
XA
=KC AO t
1−X A ---------------------(9)
The above equation is the performance equation of a batch reactor for second order reaction.
XA
Let  = C AO ( 1− X A )
Plot a graph of  Vs t, the slope of the graph is Rate constant K

PROCEDURE:
 Prepare 1 liter NaOH solution.

 Estimate the strength of NaOH solution by using standard Oxalic acid.
 Estimate the strength of HCl solution by using standardized NaOH solution.
 Transfer nearly 750 ml of NaOH solution into batch reactor.
 Take nearly 15 conical flasks and transfer 15 ml of HCl solution into each conical flask.
 Switch on the stirrer
 Add some amount of ethyl acetate to the reactor such that Ethyl acetate is maintained as limiting
reactant.
 Transfer the reaction mixture into conical flask, which contains 15 ml of known HCl solution for
every one minute time interval.
 Take the samples up to 10 minutes.
 Note down the room temperature.
 Titrate the contents of conical flask with NaOH solution to estimate the concentrations of Ethyl
Acetate and NaOH concentrations.
OBSERVATIONS
Standardization of NaOH
Volume of Oxalic acid taken = Voxalic = ml.
Normality of Oxalic acid taken = Noxalic = N
Volume of NaOH rundown for neutralization of Oxalic acid =V1= ml.
Standardization of HCl
Volume of HCl taken = V2 = ml
Volume of NaOH rundown for neutralization of HCl = V3 = ml.
Volume of reaction mixture taken into a conical flask = Vsample = ml.
Volume of Hcl taken in conical flask. = VHCl = ml.

Volume of Ehtyl Acetate added to the reactor = VEthyl = ml.
Volume of NaOH taken in to the reactor = QNaoH = ml
Time ( min ) Volume of NaOH rundown

S.No
VNaOH ( ml )
CALCULATIONS:
Standardization:
V oxalic N oxalic
Normality of NaOH solution = NNaOH = V1 = N
V 3 N NaOH
Normality of HCl solution = NHCl = V2 = N
Estimation of initial concentrations:
V Ethyl ρ
M .w
Initial concentration of Ethyl Acetate = CA0 = V =
QNaOH N NaOH
Initial concentration of NaOH = CB0 = V
Where  is the density of Ethyl Acetate
M.w is the molecular weight of Ethyl Acetate.
V is the volume of reaction mixture = QNaOH + VEthyl

Analysis of reaction mixture:
Gram moles of HCl remaining = VNaOH NNaOH
Gram moles of NaOH present in reaction mixture
GMNaOH = Gram moles of HCl used for neutralization of NaOH remaining in reaction mixture
= Gram moles of HCl added – gram moles of HCl remaining.
= VHCl NHCl - VNaOH NNaOH.
Concentration of NaOH in reaction mixture
GM NaOH
CA = CB = V sample
Conversion of Ethyl acetate
XA = 1 – ( CA / CA0)
XA
 = C AO ( 1− X A )
S.No CA CB A  Time
Plot a graph  vs time
 slope = K
time
RESULT:
The rate constant for the reaction of Ethyl Acetate with NaOH is _____________.
EXPERIMENT –II
KINETIC STUDIES IN BATCH REACTOR WITH EQUIMOLAR FEED
AIM:
To determine rate constant for the saponification by using integral analysis.
Apparatus:
Chemicals required:
NaOH solution, Ethyl Acetate, Hydrochloric acid, Phenolphthalein indicator
Theory:
The experimental batch reactor is usually operated isothermally and at constant volume, because it
is easy to interpret the results of such runs. This reactor id relatively simple device adaptable to
small-scale laboratory set-ups, and it needs but little auxiliary equipment or instrumentation. Thus, it
is used whenever possible for obtaining homogeneous data. The starting point for all design is the
material balance expressed for any reactant or product over a small element of volume.

Rate of
Rate of Rate of Rate of reactant accumulation of
reactant flow reactant flow loss due to reactant within
into element = = out of element
+ + chemical+ + the element of
of volume of volume reaction within volume
the element of
volume
If the composition within the reactor is uniform ( independent of position ), the accounting may be made
over the whole reactor. If the composition is not uniform ( dependent on position ), it must be made over a
differential element of volume and then integrated across the whole reactor for the appropriate flow and
concentration conditions.
INPUT = OUTPUT + DISAPPEARNCE BY REACTION + ACCUMULATION ----------(1)
In the batch reactor of figure 1.1 the reactants are initially charged into a container, are well mixed,
and are left to react for a certain period. The resultant mixture is then discharged. This is unsteady
state operation where the concentration changes with time. The concentration is independent of
position, so we can make material balance over the entire reactor.
Make a material balance for any component A. For such an accounting we usually select the
limiting reactant.
Input = 0
Output = 0
Disappearance by reaction (moles / time) = (-A) V

dN A d [ N AO (1− X A )] dX A
N AO
Accumulation of A (moles / time) = dt = dt = - dt
By replacing these terms in equation (1)
dX A
N AO
0 = 0 + ( -A ) V - dt
dX A
N AO
( -A ) V = dt ----------------------------------------(2)
Rearranging and integrating equation (2) gives
XA
dX A
N AO ∫
t= 0 (−γ A )V ----------------------------(3)
For constant volume reactions
XA
dX A
t=C AO ∫
0 (−γ A ) -----------------------------------------(4)
The performance equation for Constant volume batch reactor is
XA
dX A
t=C AO ∫
0 (−γ A )
Consider a second order irreversible bi-molecular elementary reaction given below
A +B Products
The rate equation for above reaction is -A = K CA CB ----------------------- (5)

Let XA and XB are conversions of A and B at any time, the concentrations of A and B at any time in
the reactor are
CA = CAO ( 1 - XA ) CB = CBO ( 1 – XB )
Substitute above expressions in equation (5)
-A = K CAO ( 1 - XA ) CBO ( 1 – XB )
Rearrange above equation
-A = K CAO ( 1 - XA ) (CBO – CBO XB ) --------------------------------------------(6)
at any time moles of B reacted is equal to moles of B reacted
moles of B reacted = CBO XB
moles of A reacted = CAO XA
CBO XB = CAO XA ----------------------------------------------------(7)
Substitute (7) in (6)
-A = K CAO ( 1 - XA ) (CBO – CAO XA )
the above equation can be rearranged as
-A = K CAO2 ( 1 - XA ) (M – XA ) ---------------------------------------(8)
C BO
where M = C AO , the initial molar ratio of reactants.
XA
dX A
t =C AO ∫
0 KC ( 1 - XA )( M-XA )
AO2
Integration of above equation leads to
1
C AO ( M −1 )
ln
[
( M −X A )
= Kt
]
M ( 1− X A ) ---------------------(9)
The above equation is the performance equation of a batch reactor for second order reaction.
1
C AO ( M −1 )
ln
[
( M −X A )
M ( 1− X A ) ]
Let  =
Plot a graph of  Vs t, the slope of the graph is Rate constant K
PROCEDURE:
 Prepare 1-liter NaOH solution.

 Estimate the strength of NaOH solution by using standard Oxalic acid.
 Estimate the strength of HCl solution by using standardized NaOH solution.
 Transfer nearly 750 ml of NaOH solution into batch reactor.
 Take nearly 15 conical flasks and transfer 15 ml of HCl solution into each conical flask.
 Switch on the stirrer
 Add some amount of ethyl acetate to the reactor such that Ethyl acetate is maintained as limiting
reactant.
 Transfer the reaction mixture into conical flask, which contains 15 ml of known HCl solution for
every one minute time interval.
 Take the samples up to 10 minutes.
 Note down the room temperature.
 Titrate the contents of conical flask with NaOH solution to estimate the concentrations of Ethyl
Acetate and NaOH concentrations.
OBSERVATIONS
Standardization of NaOH
Volume of Oxalic acid taken = Voxalic = ml.
Normality of Oxalic acid taken = Noxalic = N
Volume of NaOH rundown for neutralization of Oxalic acid =V1= ml.

Standardization of HCl
Volume of NaOH rundown for neutralization of HCl = V3 = ml.
Volume of reaction mixture taken into a conical flask = Vsample = ml.
Volume of Hcl taken in conical flask. = VHCl = ml.
Volume of Ehtyl Acetate added to the reactor = VEthyl = ml.
Volume of NaOH taken in to the reactor = QNaoH = ml
Time ( min ) Volume of NaOH rundown

S.No
VNaOH ( ml )
CALCULATIONS:
Standardization:
V oxalic N oxalic
Normality of NaOH solution = NNaOH = V1 = N
V 3 N NaOH
Normality of HCl solution = NHCl = V2 = N
Estimation of initial concentrations:
V Ethyl ρ
M .w
Initial concentration of Ethyl Acetate = CA0 = V =
QNaOH N NaOH
Initial concentration of NaOH = CB0 = V
Where  is the density of Ethyl Acetate
M.w is the molecular weight of Ethyl Acetate.
V is the volume of reaction mixture = QNaOH + VEthyl
C BO
Initial molar ratio of reactants M = C AO
Analysis of reaction mixture:

GMNaOH = Gram moles of HCl used for neutralization of NaOH remaining in reaction mixture
= Gram moles of HCl added – gram moles of HCl remaining.
= VHCl NHCl - VNaOH NNaOH.
GM NaOH
Concentration of NaOH in reaction mixture, CB = V sample
Concentration of Ethyl acetate in reaction mixture
CA = CA0 – ( CB0 – CB)
XA = 1 – ( CA / CA0)
=
ln
[
( M− X A)
M (1−X A ) ]
S.No CA CB A  time
Plot a graph  vs time
 slope = K
time
RESULT:
The rate constant for the reaction of Ethyl Acetate with NaOH is _____________.
EXPERIMENT-III
KINETIC STUDIES IN MFR
AIM:
To determine the rate constant for the saponification reaction.
THEORY:
The steady state flow reactor is ideal for industrial purposes when large quantities materials are to
be processed and when the rate of reaction is fairly high to extremely high. The starting point for all reactor
design is the material balance to be expressed for any reactant (or product)
Rate of
Rate of Rate of Rate of reactant accumulation of
reactant flow reactant flow loss due to reactant within
= + +
chemical
into element out of element the element of
of volume = of volume + reaction within + volume
the element of
volume
Where the composition within the reactor is uniform (independent of position), the accounting may be made
over the whole reactor. Where the composition is not uniform, it must be made over a differential element of
volume and then integrated across the whole reactor for the appropriate flow and concentration conditions.
The mixed flow reactor is one type of ideal steady state flow reactor. It is also called as the back mix
reactor, the ideal stirred tank reactor, or CSTR (constant flow stirred tank reactor) and, as its name
suggests, it is a reactor in which the contents are well stirred and uniform throughout. Thus the exit stream
form this reactor has the same composition as the fluid within the reactor. We refer to this type of flow as
mixed flow and the corresponding reactor, the mixed reactor, or mixed flow reactor.
The performance equation for the mixed flow reactor is obtained from equation – 1, which makes an
accounting of a given component within an element of volume of the system. But since the composition is
uniform throughout, the accounting may be made about the reactor as a whole. By selecting reactant for
consideration, equation –1 becomes
INPUT = OUTPUT + DISAPPEARANCE BY REACTION + ACCUMULATION----------------(2)
CAO
VO, FAO, XAO = o
CA,XA, FA
Fig 2.2 Continuos stirred tank reactor
As shown in Fig2.2, if FA0 = V0CA0 is the molar feed rate of component A to the reactor, then considering the
reactor as whole
Input of A moles / time = FA0(1 - XA0) = FA0
Out put of A moles / time = FA = FA0(1 - XA) = FA
( moles
Disappearance of A by reaction time
)
= (Moles of A reacting / time, volume of fluid) x (volume of reactor)
= ( - A ) V
Accumulation is zero because of steady state operation
Substitute above in equation (2), we obtain
FA0 - FA0(1 - XA) + (-A) V------------------------- (3)
FA0 XA = ( - A) V -------------------------- (4)
Which on re-arranging
V X
= A
F AO −γ A
substitute FA0 = V0CA0 in above equation
V X
= A
V O C AO −γ A
V
Substitute space time  = v O in above equation
τ X
= A
C AO −γ A
The performance equation for CSTR is

V τ X
= = A
F AO C AO −γ A ---------------------------------------(5)
Where XA and - A are evaluated at exit stream conditions, which are the same as the conditions with in the
CA
reactor. For the special case of constant density systems X A = 1- C AO , in this case the performance
equation of Mixed flow reactors can also be written in terms of concentrations, or
V τ XA C AO −CA
= = =
F AO C AO −γ A C AO (−γ A ) --------------------------(6)
or
C AO −C A
τ=
−γ A --------------------------------------(7)
The above is the performance equation for CSTR for constant density systems.
Consider the second order irreversible bi-molecular type reaction
A+B Products
dC A dC B
= =
With corresponding rate equation -γ A = - dt - dt K CA CB --------------(8)
Noting that the amounts of A and B which have reacted at any time t are equal and given by C AO XA = CBO
XB then equation (8) becomes
dC A dC B
γ = =
- A = - dt - dt K (CAO - CAOXA) (CBO - CAOXA)
= K CAO2 (1- XA) (M - XA) ----------------------(9)
substitute (9) in (7)

XA
Kτ=
C AO (1− X A )( M − X A ) --------------------------------(10)
The above is the performance equation for second order, bimolecular irreversible in Continuous Stirred
Reactor.
Procedure:-
 Transfer NaOH and ethyl acetate solutions into overhead tanks

 Estimate strength of NaOH using 0.1N Oxalic acid
 Estimate strength of HCl using NaOH
 Adjust the flow rates of ethyl acetate NaOH ( Keep Ethyl Acetate as limiting reactant )
 Note down the flow rates after steady state has attained
 Collect 10ml of reaction mixture from outlet and transfer it into a conical flask which
contains15ml of HCl
 Titrate it against NaOH
 Repeat the same experiment for different flow rates and tabulate readings
 Note down the room temperature
OBSERVATIONS:
Standardisation of NaoH solution:
Volume of Oxalic acid taken = V1= ml
Normality of Oxalic acid taken = N1= ml
Volume of NaOH rundown against oxalic acid = V2= ml
Standardisation of HCl:
Volume of HCl taken = V3= ml
Volume of NaOH rundown against HCl = V4= ml
S.No Flow rate of NaOH Flow rate of Ethyl Volume of NaOH rundown
solutionQNaOH (Lph) Acetate QEA (Lph) VNaOH (ml)
Volume of reaction mixture taken from reactor = Vsample= ml
Volume of HCl taken into conical flask = VHCl= ml
Volume of Ethyl Acetate added per litre of water = VEA = ml
Density of Ethyl Acetate =  = g/cc
Volume of reactor V = Lt
CLACULATIONS:
N 1V 1
Normality of NaoH solution = NNaOH = V2
N NaOH V 4
Normality HCl solution = NHCl = V3
QNaOH N NaOH
Initial concentration of NaOH, CBO = Q NaOH +QEA
V EA ρ
Strength of Ethyl Acetate solution = SEA = M . W ( 1+V EA )
Q EA S EA
Initial concentration of Ethyl Acetate solution = CAO = QNaOH +Q EA
Gram moles of HCl added = VHCl NHcl
Gram moles of HCl remaining

= gram moles of NaOH used for back Titration
= VNaOH NNaOH
Gram moles of NaOH remaining in the reaction mixture ( GNaOh)
= Gram moles of HCl utilized
= VHCl NHcl - VNaOH NNaOH
G NaOH
Concentration of NaOH, CB
V
= sample
CB
Conversion of NaOH = XB = 1 - C BO
Conversion of Ethyl Acetate, XA = M XB
XA
C (1− X A )( M− X A )
 = AO
V
Residence time =  = QNaOH +Q EA
Repeat the above calculations for all flow rates.
GRAPH: - Plot a graph between τ Vs 

Rate constant = slope
RESULT: -
The rate constant for the saponification reaction is K = -----------
EXPERIMENT-IV
KINETIC STUDIES IN PFR
AIM:
To determine the rate constant for the saponification reaction.
THEORY:
The steady state flow reactor is ideal for industrial purposes when large quantities material are to be
processed an d when the rate of reaction is fairly high to extremely high.
The starting point for all design is the material balance expressed for any reactant (or product)
Element of reactor
volume
Reactant leaves
Reactant enters
R eactant accumulates Reactant disappears by

rate of reactant rate of reactant rate of reactant rate of reactant
flow into flow out of loss due to chemical accumulation of
element of = element of + reaction within the + reactant in
volume volume element of volume element of volume
Where the composition within the reactor is uniform (independent of position), the accounting may be
made over the whole reactor. Where the composition is not uniform, it must be made over a differential
element of volume and then integrated across the whole reactor for the appropriate flow and concentration
conditions.
The first of the two ideal steady state flow reactors is variously known as the plug flow, slug flow, piston
flow, ideal tubular, and unmixed flow reactor, and it is shown in fig 3.1
feed Fig. 3.1 Plug flow reactor product
We refer to it as plug flow reactor and to this pattern of flow as plug flow. It is characterized by the fact that
the flow of fluid through the reactor is orderly with no element of fluid over taking or mixing with any other
element ahead or behind. The necessary and sufficient condition for plug flow is for the residence time in
the reactor to be same for all elements of fluid.
In a plug flow reactor the composition of the fluid varies from point to point along a flow path; consequently,
the material balance for a reaction component must be made for a differential element of volume dV. Thus
for reactant A equation (1) becomes
Input = output + disappearance by reaction + accumulation --------(2)

where
CA = concentration of reactant A
FA = molar flow rate of A
A = conversion of A
O = volumetric flow
A = rate of reaction.
Subscript 0 indicates entering, subscript f indicates leaving conditions.
As shown in fig 3.2., consider a small element of volume dV in the reactor and apply equation (2) over
small element of volume dV
Input of A moles / time = FA
Output of A moles / time = FA + dFA
Disappearance of A by reaction moles / time
= (moles of A reacting / time, volume of fluid)(volume of reactor)
= (-A) dV
Accumulation is Zero because of steady state operation
Substitute above in equation (2), we obtain
FA = (FA + dFA) + (-A) V ---------------------(3)
dFA = (-A) dV ---------------------(4)
FA = FAO(1- A)
From above equation d FA = FAO dA ---------------------(5)

FAO dA = (-A) dV ---------------------(6)
This, then, is the equation accounting for A in the differential section of reactor of volume dV. For the
reactor as a whole the expression must be integrated. Now F AO the feed rate, is constant, but -A is
certainly dependent on the concentration of materials and conversion. Grouping the terms accordingly, we
obtain
X Af
V
dX A
∫ FdVAO ∫ −ϒ A
O = 0
Thus
X Af
dX A
V τ ∫ −ϒ A
F A0 = C A0 = 0 ----------------------------------------(8)
X Af
dX A
or
∫ −ϒ A
 = CAO 0
------------------------------------------(9)
The above is the performance equation for plug flow reactor.
The reaction between Ethyl acetate and NaOH is bimolecular second order reaction type given below
A + B Products
With rate equation -A = K CA CB
At any time moles of A reacted is same as moles of B reacted
CAOXA = CBOXB
Then -A = K CAO2 ( 1 - XA ) ( M – XA )
Substitution of above equation in (9) and integration leads to

[( M −X A )
ln M (1− X A )
] = K CAO ( M – 1 ) 
- -----------------------(10)
1
[
( M −X A )
C AO ( M - 1 ) ln M (1− X A ) ] = K
----------------- ( 11 )
PROCEDURE:
1. Transfer NaOH and Ethyl acetate solutions into overhead tanks.

2. Estimate the strength of NaOH solution by using standard Oxalic acid.
3. Estimate the strength of HCl solution with the help of NaOH solution.
4. Adjust the flow rates of Ethyl acetate and NaOH solutions into PFR.
5. Note down the flow rates after steady state has attained
6. Collect 10 ml of reaction mixture from the reactor outlet.
7. Transfer the reaction mixture into a conical flask containing 15 ml of 0.1 N HCl solution.
8. Titrate above mixture against NaOH solution
9. Repeat the experiment for different flow rates and tabulate the readings.
10. Note down the room temperature.
OBSERVATIONS:
STANARDISATION OF NaOH
Volume of Oxalic acid taken = Voxalic = ml
Normality of Oxalic acid = Noxalic = N
Volume of NaOH rundown for neutralization of Oxalic acid = V1 = ml
STANDARDISATION OF HCl
Volume of NaOH rundown for neutralization of HCl = V3 = ml
S.No Flow rate of Flow rate of NaOH VB Volume of NaOH rundown

Ethyl acetate ( cc / time) for back titration VNaOH
VA ( cc / time)
Volume of reaction mixture taken into conical flask = ml
Volume of HCl taken in conical flask = VHCl = ml
CALCULATIONS:
Normality of NaOH solution = NNaOH = Voxalic x Noxalic / V1 = N
Normality of HCl solution = NHCl = V3 x NNaOH / V2 = N
Strength of Ethyl acetate = CAS = Q x  / MW x V
Where
Q = Volume of Ethyl acetate added in one liter of water
 = Density of Ethyl acetate ( gm / cc)
MW = Molecular weight of Ethyl acetate
V = volume of solution = volume of water + volume of Ethyl acetate added ( cc )
Volumetric flow rate of Ethyl acetate = VA = cc / time.
Volumetric flow rate of NaOH = VB
Initial concentration of Ethyl acetate CAO = CAS VA / ( VA + VB )

Initial concentration of NaOH solution CBO = NNaOH VB / ( VA + VB )
M = CBO / CAO
GMNaOH = Gram moles of HCl used for neutralization of NaOH
remaining in reaction mixture
= VHCl NHCl - VNaOH NNaOH
Concentration of NaOH in reaction mixture
CB = GMNaOH / volume of reaction mixture taken
Concentration of Ethyl acetate in reaction mixture
CA = CAO – ( CBO – CB )
A = 1 – ( CA / CAO )
1
[
( M −X A )
 = C AO (M −1) ln M (1− X A )
]
Space time = volume of reactor / ( VA + VB )
S.No CA CB A  
Plot a Graph  Vs 
From the above graph, Rate constant  = Slope of the line
RESULT:
The rate constant for the saponification reaction is ________________

EXPERIMENT-V
ISOTHERMAL BATCH REACTOR
AIM:
To Study of a Non – Catalytic Homogeneous reaction in an isothermal batch reactor.
To determine the reaction rate constant (K) for the given saponification Reaction of ethyl acetate in
aqueous sodium hydroxide solution.To study the effect of temperature on k and determine the activation
energy description
A batch reactor is closed system with no input and output streams. A batch reactor can operate under
conditions like isothermal (Temperature of reaction Mass remains constant), perfectly mixed (composition
of reaction mixture is uniform throughout), and constant volume (volume of the reaction mixture within the
reactor remains const, there is no appreciable change in the density of reaction mass). This set – up is
used to study a non – catalytic homogeneous reaction under isothermal condition
The set up consists of a reactor fitted in a constant temperature water bath. One stirrer is fitted for mixing
the reactants in reactor and other is fitted in water batch to keep the uniform temperature throughout in the
bath. The temperature of bath can be maintained from ambient to 90 0C with the help of Digital temperature
indicator cum controller. Samples can be taken out with the help of a sampling pipette.
Volume of reactor = 2.815lts
Volume of bath = 14.3lits
Reactor stirrer=100rpm
Bath stirrer – 100rpm
Temperature controller – ambient to 2000C with 10C resolution
UTILITIES REQUIRED
1. Water supply
2. Drain
3. Electricity supply 1 phase 220V AC, 1.5kw
4. Instruments, laboratory glass ware and chemicals required for analysis as per the system adopted.
CHEMICALS:
1. N/10 NaOH
2. N/10 HCl
3. N/10 Ethylacetate (8.8gms of ethyl acetate in 1 lits of water), indicator (phenolphthalein)
EXPERIMENTAL PROCEDURE:
1. Prepare a solution of N/10 ethyl acetate by mixing 8.8gms (or 9.8ml at 20 0C) of ethyl acetate in 1L
of solution.
2. Prepare a solution of N/10 NaOH by dissolving 4gms / 1L of solution
3. Prepare a solution of N/10 HCl
4. Use phenolphthalein as indicator
5. Take 6Nos of 250ml beakers and put 20ml of N/10HCl in each beaker
6. Take N/10 NaOH in the burette
7. Adjust the temperature of water bath at 250C
8. If the volume of reactor is 1L then take 1000ml each of N/10 CH 3COOC2H5 and N/10 NaOH in two
separate flasks and keep these in the water bath for about 15min
9. Transfer these solutions quickly in the batch reactor. Start immediately the mixer and the stop
watch
10. At regular intervals of 1-2 min withdraw 10ml of reaction mixture and put it in the marked beakers
containing N/10HCl. Take at least 6 samples at regular interval of time
11. Transfer the solution from beakers to the conical flasks, and titrate the excess N/10 HCl in each
flask using N/10 NaOH from burette and phenolphthalein as indicator
12. Record the reaction temperature
13. In order to study the effect of temperature on k the above steps may be repeated at temperature =
350C and 500C. All the reactants must be preheated in the water batch before mixing in the reactor.
OBSERVATIONS AND CALCULATIONS
o
Temperaure = C
Normality of Ethyl acetate = N/10
Normality of NaOH = N/10
Volume of Ethyl acetate taken = 1000ml
Volume of Sodium Hydroxide = 1000ml
S. No Time, t Min. Volume of NaOH rundown
For back titration( VNaOH)
CALCULATIONS:
Initial concentration of NaOH CAO = 0.05 N

Initial concentration of Ethyl Acetate CBO = 0.05 N
Concentration of NaOH at any time CA = (0.1x VNaOH – NHCl x VHCl)/10
Time (t) 1/CA

Plot 1/CA versus timeFor second order reaction for equimolar feed the performance equation is
1/CA
Time, t
1 1
= +kt
C A C AO
From the above graph rate constant ‘k’ = slope of line

Repeat the above calculation procedure for different temperatures and calculate the rate constants
Tabulate k values at 3 or 4 different temperatures
S. NO Temperature Rate constant I/T
T, K K
Plot k Vs 1/T on a semi log graph
EA
Slope =−
R
Intercept = k0
Express, k = k0 e – EA/RT
Standard Data
Reactor : Material stainless steel 304 grade, Volume 2.1Lts(Approx)
Water Bath : Material stainless steel 304 grade, double wall, insulated with
ceramic wool
Heater : Nichrome wire Heater
Stirrers (2Nos) : stainless steel 304 grade impeller and shaft coupled with FHP
motor
Stop watch : electronic
Temperature sensor : RTD PT – 100 type
Control panel comprises of Digital Temperature controller cum – indicator ( For Batch) = 0 – 1999.9 0C,
RTD PT – 100 type
With standard make on/off switch, mains indicator fuse etc
The whole unit is assembled rigidly on a base plate and mounted on a stand
Most of the parts are powder coated and rest are painted with auto paints
PRECAUTIONS & MAINTANANCE INSTRUCTION:
1. Measure the exact volume of water and weigh the chemicals

2. Always use clean water and good quality chemicals and standard solution for titration
3. Use electronic balance for weighing of chemicals. Don’t mix the droppers of different chemicals
4. Keep close all the drain valves and vent valve should open while filling the reactant in feed tanks
5. Flow should not be disturbed during the experiments
6. Handle the chemicals carefully
7. Don’t switch ON heater before filling the water in the bath
8. There should be no air in the flow during experiment
Result : The activation energy of the given reaction is ____________.
EXPERIMENT-VI
KINETIC STUDIES IN ADIABATIC REACTOR
Aim:
To study of a catalytic homogeneous reaction in a batch reactor, under adiabatic condition.
To study the hydrolysis of acetic anhydride with water in presence of an acid catalyst (H2SO4)
To predict the degree of conversion from time – temperature data.
THEORY:
Industrial scale chemical reactions are frequently complicated by variations occurring in the temperature of
the reactor during operation. Temperature changes always effect the physical properties of the reaction
mixture and the reaction rate constant. The temperature dependence specific reaction rate constant, k is
expressed in terms of Arrhenius equation as:
k =k 0 e−E /RT
In case of an exothermic reaction, the heat relieved by the chemical reaction increases the reaction
temperature, which in turn increases the reaction rate constant and hence the rate of reaction. Degree of
conversion, x, is correspondingly effected.
For non – isothermal operation of a batch reactor, the analysis is carried out by using the basic material
balance equation in conjunction with an energy balance and an Arrhenius type expression for the reaction
rate.
REACTION
(CH3CO)2O + H2O CH3COOH
The energy balance around the reactor is:
Heat transfer from surroundings = heat of reaction + energy accumulation in reactor
On substituting corresponding quantities the energy equation is:

U A(Ts – T) dt = r VR H dt + MT CPav dT
In terms of conversion it is expressed as:
U A(Ts – T) dt = r MA H dx + MT CPav dT
Where U is the overall heat transfer coefficient between the reactor surface and the ambient atmosphere
A is the heat transfer area,
Ts is the temperature of the heating or cooling medium,
T is the temperature of the reaction mixture.
VR is the reaction volume,
H is the heat of reaction
r is the rate of reaction
t is the time.
X is the fractional conversion = mass of A reacted / initial mass of ractant A
MT is the total reaction charge,
CPav is the average specific heat of the reaction mass
MA is the initial moles of the reactant A
FOR AN ADIABATIC PROCESS:
The energy equation reduces to:
- MA H dx = MTCPav dT
On integration this equation gives:
T = T0 – (MA H / MTCPav ) x
Or T = T0 -  x
Where T0 is the initial batch temperature at x = 0

 = (MA H / MTCPav )
and corresponding batch time of first order reaction is given by:
t=C A 0 ∫ dx/[kC A 0 (1−x)]
xf
t=C A 0 ∫ dx /[k (1−x )]
or 0
−E /RT
Where k =k 0 e
From the observed values of temperature (T) as a function of time (t), degree of conversion, x is obtained
from equation (2) and corresponding reaction rate constant, k is obtained from equation (5). Knowing k and
x, the required batch time for the first order reaction for the desired degree of conversion x f is obtained from
equation (4). Equation (4) can be solved graphically or by R – K method
REACTION TO BE STUDIED IN THIS EXPERIMENT IS THE “HYDROLYSIS OF ACETIC ANHYDRIDE

WITH WATER USING H2SO4 AS CATALYST
THE REACTION IS
(CH3CO)2O + H2O CH3COOH
(The reaction takes place in presence of solvent acetic acid and is of FIRST ORDER)
properties of the reActants:
Acetic Anhydride : (CH3CO)2O, M.W. = 102.09, density at 200C (A) = 1.082gm/cc
Acetic Acid : CH3COOH, M.W. = 60.05, density at 200C (A) = 1.049gm/cc
Water : H2O, M.W. = 18.01, density at 200C (A) = 1gm/cc
Heat of reaction = (- H) = 58.562J/gmol of acetic anhydride reacted
Reaction rate constant, k for this reaction is expressed as ln(k) = 16.0502 – 5344.5 / T, Where T is the
reaction temperature in degree K and k is in min-1
Average specific heat of the reaction mixture may be taken as: Cpav = 3768.3Jkg-K
DESCRIPTION:
The adiabatic batch reactor consists of a Dewar flask of capacity 1L, fitted with a stirrer and a Pt – 100
temperature sensor and a stop watch. The temperature is indicated by a digital temperature indicator.
UTILITIES REQUIRED:
CHEMICALS:
1. Acetic Anhydride
2. Acetic Acid
3. Distilled Water
4. Sulphuric Acid
EXPERIMENTAL PROCEDURE:
1. Prepare an initial charge as given below:
Solution A
Acetic Anhydride = 200ml
Acetic Acid = 300ml
Solution B
Water = 210ml
H2SO4 =0.1%(wt) of water
2. Set the stirrer speed around 60 – 70ppm,

3. Start the temperature indicator (please calibrate Pt – 100 sensor with a Beckman Thermometer, if
available)
4. Put solution A and Solution B simultaneously into the reactor and start the stop watch
5. Record the reaction temperature immediately after the reactor has been loaded at t = 0, This is T0
6. Record time – temperature data ( t Vs T) till you pass the maximum. It shall be around 600C
7. Stop the stirrer, close the temperature indicator and gently remove the contents of the reaction
mixture, wash the reactor with water.
STANDARD DATA:
Reactor = Material Stainless Steel 304 grade, Capacity 1Ltrs,
(Approx) Insulated with Ceramic wool.
Stirrer = Teflon Impeller and Stainless Steel shaft coupled with FHP motor
Control panel comprises of =
Digital temperature indicator = 0 – 199.90C, RTD PT – 100type
Temperature Sensors = RTD PT – 100 type
With standard make on/off switch, Mains Indicator etc,
The whole unit is assembled rigidly on abase plate and mounted on a stand.
Most of the parts are powder coated and rest are painted with auto paints.
Volume of acetic anhydride taken = 200ml
Volume of acetic acid taken as solvent for acetic anhydride = 300ml
Volume of acidified water (H2SO4 = 0.1%wt) = 210ml
OBSERATIONS:
S.No. Reaction Time, t, min Reaction Temp, T, 0C
5
6
10
11
12
RESULT:
The activation energy of the given reaction is ____________.

EXPERIMENT-VII
RTD STUDIES IN MFR
AIM:
To determine the non-ideality of reactor through its dispersion number and comparison of
residence time distribution with ideal reactor.
APPARATUS:
CHEMICALS REQUIRED:
NaOH solution, Ethyl Acetate, HCl, Phenolpthaline indicator
THEORY:
Single CSTR RTD : In a CSTR the concentration of any substance in the effluent stream is
identical to the concentration throughout the reactor. A material balance on an inert Tracer that
has been injected as a pulse into a CSTR yields
IN - OUT = ACCUMULATION.
dC
0 – v C = V dt
Separating the variables and integrating with C = C0 at t=0 yields
t
−
τ
C(t) = C O e
C (t )
E(t )= ∞ −
t
∫ C (t )dt
τ
e
The Exit age distribution of ideal CSTR 0 = τ
In many CSTRs, the outlet and inlet pipes are close together, so some short-circuiting occurs. In
addition to short-circuiting, stagnant regions (dead zones) are often encountered. In these regions
there is little or no exchange of material with well-mixed regions, and consequently virtually no
reaction there.
Measurement of RTD :
The RTD is determined experimentally by injecting inert chemical molecule or atom, called a tracer
into the reactor at some time t=0 and then measuring the tracer concentration, C, in the effluent
stream as function of time. The two most used methods of injection are pulse input and step input.
Pulse input: In a pulse input, an amount of tracer N0 is suddenly injected in one shot into the feed stream
entering the reactor in as short a time as possible. The outlet concentration is then measured as a
function of time. Choose an increment of time t sufficiently small that the concentration of tracer,
C(t), exiting between time t and t+t is essentially constant.
The amount of tracer material, N, leaving the reactor between time t and t+t is then
N = C(t) v t ----------(1) where v is volumetric flow rate.
In other words, N is the amount of material that has spent an amount of time between t and t+t
in the reactor.
Divide (1) by the total amount of material that was injected into the reactor, NO
ΔN C (t )vΔt
=
NO NO ----------(2)
which represents the fraction of material that has a residence time in the reactor between t and
t+t.
vC (t )
For impulse input we define E(t) = N O , substitute this in (2)
ΔN
=E (t ) Δt
NO ------------------(4)
The quantity E(t) is called the residence time distribution function. If NO is not known directly, it can
be obtained from the out let concentration measurements by summing up all the amounts of
materials, N, between time equal to zero and infinity.
∞
∫ vC (t )dt
N0 = 0
The volumetric flow rate usually constant, so we can define E(t) as
C (t )
E(t )= ∞
∫ C (t )dt
0
The integral in the denominator is the area under the C curve.
Is very common to compare RTDs by using their moments instead of trying to compare their entire
distributions. For this purpose, three moments are normally used. The first is the mean residence
time, the second moment commonly used is taken about mean is called variance, or square of the
standard deviation. The third moment also taken about the mean and is related to skewness.
Mean residence time of molecules in the reactor t is given by
∞
t=∫ tE(t )dt
0
The variance is defined by
∞
σ =∫ ( t−t ) E(t )dt
2 2
σ2
σ 2=
θ t2
Based on dimensionless variance non-ideal reactors can be modeled based on RTD. The
one-parameter models of non-ideal reactors are
1. Dispersion model
2. Tanks in series model
The Dispersion number for ideal plug flow reactor is zero.
The Dispersion number for ideal mixed flow reactor is .
The dispersion number for closed-closed vessel boundary conditions is given by the equation
( ) ( ) (1−e )
2 uL
−
D D D
σ 2 =2 −2
θ uL uL
The dispersion number for open vessel boundary conditions is given by the equation
( ) ( )
2
D D
σ 2 =2 +8
θ uL uL
If the Dispersion number is < 0.1 the flow is nearly plug flow
If the Dispersion number is between 0.1 and 10, the flow is intermediate
If the Dispersion number is >10 the flow is nearly mixed flow
PROCEDURE:
 Standardise the NaOH solution using Oxalic acid.

 Adjust some flow rate of water to the reactor and allowed the system foe steady state.
 After the system reaches steady state, note down the flow rate of stream into the reactor.
 Inject Glacial acetic acid as a tracer.
 Collect 10 ml from exit stream of each 30 sec interval.
 Titrate each sample against NaOH, and note down the volume of NaOH rundown.
 Collect the samples till there is no Acetic acid present in the exit stream.
 Note down the volume of reactor.
OBSERVATIONS:
Standardization of NaOH :
Volume of Oxalic acid taken (V1) = ml
Normality of Oxalic acid taken (N1) = N
Volume of NaOH rundown for Nuetralization = V = ml.

Time, t min Volume of NaOH
Rundown VNaOH
Volume of Sample collected from exit stream = 10 ml.
Volume of reactor = VM = lt.
Volumetric flow rate to the reactor VO = Lph.
CALCULATIONS:
V 1 N1
Normality of NaOH = NNaOH = V
VM
x 60
Residence time in the reactor  = V O min.
V NaOH N NaOH
Concentration of Acetic acid in the exit stream at time t, C(t) = 10
Plot a graph C(t) Vs t

∞
∫ C (t )dt
Q= 0 = Area under the Curve C(t) Vs t
C(t )
The Exit age distribution function at time t, E(t) = Q
Plot a graph of E(t) Vs t
∞
t=∫ tE(t )dt
The mean Residence time, 0
Plot a graph of tE(t) Vs t

∞
t=∫ tE(t )dt
0 = Area under the curve of tE(t) Vs t
∞
σ =∫ ( t−t )2 E(t )dt
2
The variance, 0
2
Plot a graph of ( t−t ) E(t ) Vs t
∞
σ =∫ ( t−t ) E(t )dt
2 2
2
0 = Area under the Curve ( t−t ) E(t ) Vs t
σ2
σ 2= 2
Calculate, θ t
( ) ( )
2
D D
σ 2 =2 +8
θ uL uL
Time C(t) E(t) t E(t) t2 E(t) E(t)ideal
RESULT:
1. The type of flow in the reactor is ___________________.
2. The experimental Exit age distribution is compared with ideal distribution.
EXPERIMENT-VIII
RTD STUDIES IN MFRs IN SERIES
AIM:
residence time distribution with ideal reactors.
APPARATUS:
Reactor vessels with stirrer, Conical flasks, Burette, Pipette, test tubes.
CHEMICALS REQUIRED:
THEORY:
The residence time distribution for N continuous stirred tank reactors in series is given by
E( t )=
t N −1 −
e
( )
t
τi
( N −1 )! τ N
i
PROCEDURE:

 Switch on the stirrer
 Collect 10 ml from exit stream of each 1min time interval.
OBSERVATIONS:
Volume of NaOH
Time, t
Rundown VNaOH
min
Volume of mixed flow reactor = VM = lt.
CALCULATIONS:
V 1 N1
V NaOH N NaOH

∞
∫ C (t )dt
C(t )

∞
t=∫ tE(t )dt

∞
t=∫ tE(t )dt
∞
σ =∫ ( t−t )2 E(t )dt
2
The variance, 0
2
∞
σ 2=∫ ( t−t )2 E(t )dt 2
σ2
σ 2= 2
Calculate, θ t
Number of ideal equal to this variance is given by
N = 1/2
Calculate E(t) theoretical by
VM
x 60
Residence time in the mixed flow reactor i = V O min.
N = 3.
E( t )=
t N −1 −
e
( )
t
τi
( N −1 )! τ N
i
RESULT:
1. Number of ideal equal to this variance is ____________.

EXPERIMENT –IX
RTD STUDIES IN PFR
AIM:
APPARATUS:
CHEMICALS REQUIRED:
THEORY:
The RTDs in ideal plug flow reactors is the simplest to consider. In an ideal plug flow reactor,
all the atoms of material leaving the reactor have spent precisely the same amount of time within the
reactor. The distribution function in such a case is a spike of infinite height and zero width, whose area is
V
equal to 1; the spike occurs at t =  = v . Mathematically it is represented by the Dirac delta function.
E(t)=(t-)
In  Out 
The dirac delta function are
(x) = 0, when x¿ 0. ¿
(x) =  when x = 0. E(t)
The function is illustrated in fig.1

0  time
Fig.1 Plug Flow response to a pulse tracer input
The non idealities in plug flow reactor is the axial mixing
Measurement of RTD :
The RTD is determined experimentally by injecting inert chemical molecule or atom, called a
tracer into the reactor at some time t=0 and then measuring the tracer concentration, C, in the
effluent stream as function of time. The two most used methods of injection are pulse input and
step input.
Pulse input: In a pulse input, an amount of tracer N0 is suddenly injected in one shot into the feed stream
entering the reactor in as short a time as possible. The outlet concentration is then measured as a
function of time. Choose an increment of time t sufficiently small that the concentration of tracer,
C(t), exiting between time t and t+t is essentially constant.
The amount of tracer material, N, leaving the reactor between time t and t+t is then
N = C(t) v t ----------(1) where v is volumetric flow rate.
In other words, N is the amount of material that has spent an amount of time between t and t+t
in the reactor.
Divide (1) by the total amount of material that was injected into the reactor, NO
ΔN C (t )vΔt
=
NO NO ----------(2)
which represents the fraction of material that has a residence time in the reactor between t and
t+t.
vC (t )
For impulse input we define E(t) = N O , substitute this in (2)
ΔN
=E (t ) Δt
NO ------------------(4)
The quantity E(t) is called the residence time distribution function. If NO is not known directly, it can
be obtained from the out let concentration measurements by summing up all the amounts of
materials, N, between time equal to zero and infinity.
∞
∫ vC (t )dt
N0 = 0
The volumetric flow rate usually constant, so we can define E(t) as
C (t )
E(t )= ∞
∫ C (t )dt
0
The integral in the denominator is the area under the C curve.
Is very common to compare RTDs by using their moments instead of trying to compare their entire
distributions. For this purpose, three moments are normally used. The first is the mean residence
time, the second moment commonly used is taken about mean is called variance, or square of the
standard deviation. The third moment also taken about the mean and is related to skewness.
Mean residence time of molecules in the reactor t is given by
∞
t=∫ tE(t )dt
0
The variance is defined by
∞
σ =∫ ( t−t ) E(t )dt
2 2
σ2
σ 2=
θ t2
Based on dimensionless variance non-ideal reactors can be modeled based on RTD. The one-
parameter models of non-ideal reactors are
1. Dispersion model
2. Tanks in series model
The Dispersion number for ideal plug flow reactor is zero.
The Dispersion number for ideal mixed flow reactor is .
( ) ( ) (1−e )
2 uL
−
D D D
σ 2 =2 −2
θ uL uL
( ) ( )
2
D D
σ 2 =2 +8
θ uL uL

PROCEDURE:

 After the system reaches steady state, note down the flowrate of stream into the reactor.
 Collect the samples till there is no Acetic acid present in the exit strem.
OBSERVATIONS:
Time, t Volume of NaOH

min
Rundown VNaOH
Volume of reactor = VP = lt.
CALCULATIONS:
V 1 N1
VP
x 60
Residence time in the reactor  = V O min.
V NaOH N NaOH

∞
∫ C (t )dt
C(t )

∞
t=∫ tE(t )dt
∞
t=∫ tE(t )dt
∞
σ =∫ ( t−t )2 E(t )dt
2
The variance, 0
2
∞
σ 2=∫ ( t−t )2 E(t )dt 2
σ2
σ 2=
Calculate, θ t2
( ) ( )( )
uL
−
D D
σ 2 =2 −2 1−e D
θ uL uL
Time C(t) E(t) t E(t) − E(t)ideal

(t- t )2 E(t)
RESULT:

EXPERIMENT –X
RTD STUDIES IN COMBINED REACTOR
AIM:
APPARATUS:
Reactor vessels with stirrer, Conical flasks, Burette, Pipette, test tubes.
CHEMICALS REQUIRED:
THEORY:
The residence time distribution for Combined reactor shown below is given by
( t −τ P)
−
1 τM
E( t )= e
τM when t τ P
E(t) = 0; when t 
τP
( ) ( ) (1−e )
2 uL
−
D D D
σ 2 =2 −2
θ uL uL
PROCEDURE:

 Note down the volume of both reactors.
OBSERVATIONS:
Volume of NaOH
Time, t
Rundown VNaOH
min

Volume of plug flow reactor = VP = lt.
Volume of mixed flow reactor = VM = lt.
CALCULATIONS:
V 1 N1
V NaOH N NaOH

∞
∫ C (t )dt
C(t )

∞
t=∫ tE(t )dt

∞
t=∫ tE(t )dt
∞
σ =∫ ( t−t )2 E(t )dt
2
The variance, 0
2
∞
σ 2=∫ ( t−t )2 E(t )dt 2
σ2
σ 2= 2
Calculate, θ t
D 2
( ) ( )
2
D
σ 2 =2 +8
θ uL uL
VP
x 60
Residence time in the plug flow reactor P = V O min.
VM
x 60
Residence time in the mixed flow reactor M = V O min.
Calculate E(t) theoretical by
( t −τ P)
1 − τM
E( t )= e
τM when t τ P
E(t) = 0; when t  τ P
RESULT:

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Biochemical Reaction Engineering Lab Manual

Vignan’s Foundation for Science, Technology and Research

Biochemical Reaction Engineering

3 Kinetic studies in Mixed flow reactor CO2,CO4,CO9 PSO1

4 Kinetic Studies in Plug flow reactor CO2,CO4,CO9 PSO1

5 Kinetic Studies in Isothermal Batch reactor CO2, CO4,CO7 PSO1

6 Kinetic Studies in Adiabatic reactor CO1, CO2,CO7 PSO1

7 RTD studies in Mixed flow reactor CO3, CO2,CO9 PSO1

8 RTD studies in Mixed flow reactors in series CO2,CO4,CO10 PSO1

9 RTD studies in Plug flow reactor CO1, CO2,CO7 PSO1

10 RTD studies in Combined reactor CO1, CO2,CO7 PSO1

Vision and Mission of the Program

Course Description and Objective:

KINETIC STUDIES IN BATCH REACTOR EQUIMOLAR FEED

To determine rate constant for the saponification by using Equimolar feed.

Reactor vessel with stirrer, Conical flasks, Burette, Pipette.

NaOH solution, Ethyl Acetate, Hydrochloric acid, Phenolphthalein indicator

Element of reactor volume

Reactants enters Reactants leaves

Reactant accumulates Reactant disappears by

within the element reaction within the element

INPUT = OUTPUT + DISAPPEARNCE BY REACTION + ACCUMULATION ----------(1)

Disappearance by reaction ( moles / time ) = ( -A ) V

By replacing these terms in equation (1)

Rearranging and integrating equation (2) gives

for constant volume reactions

The performance equation for Constant volume batch reactor is

Consider a second order irreversible bi-molecular elementary reaction given below

The rate equation for above reaction is -A = K CA CB (5)

Substitute above expressions in equation (5)

-A = K CAO ( 1 - XA ) CBO ( 1 – XB )

Rearrange above equation

-A = K CAO ( 1 - XA ) (CBO – CBO XB ) --------------------------------------------(6)

at any time moles of B reacted is equal to moles of B reacted

moles of B reacted = CBO XB

moles of A reacted = CAO XA

CBO XB = CAO XA ----------------------------------------------------(7)

Substitute (7) in (6)

-A = K CAO ( 1 - XA ) (CBO – CAO XA )

For equimolar feed CAO = CBO M = 1

-A = K CAO2 ( 1 - XA )2 ---------------------------------------(8)

Substitute equation (8) in equation (4)

Integration of above equation leads to

Plot a graph of  Vs t, the slope of the graph is Rate constant K

 Prepare 1 liter NaOH solution.

Volume of Oxalic acid taken = Voxalic = ml.

Normality of Oxalic acid taken = Noxalic = N

Volume of NaOH rundown for neutralization of Oxalic acid =V1= ml.

Volume of HCl taken = V2 = ml

Volume of NaOH rundown for neutralization of HCl = V3 = ml.

Volume of reaction mixture taken into a conical flask = Vsample = ml.

Volume of Hcl taken in conical flask. = VHCl = ml.

Volume of NaOH taken in to the reactor = QNaoH = ml

Time ( min ) Volume of NaOH rundown

Estimation of initial concentrations:

Where  is the density of Ethyl Acetate

M.w is the molecular weight of Ethyl Acetate.

V is the volume of reaction mixture = QNaOH + VEthyl

Gram moles of HCl remaining = VNaOH NNaOH

Gram moles of NaOH present in reaction mixture

= Gram moles of HCl added – gram moles of HCl remaining.

= VHCl NHCl - VNaOH NNaOH.

Concentration of NaOH in reaction mixture

Conversion of Ethyl acetate